ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Pyridine → 1-(6-Acetyl-4-chloro-3',5'-difluoro-3-methylbiphenyl-2-yl)pyrrolidin-2-one

HRID 510838
ノート
印刷プレビュー

反応式

HRID 510838 の反応式
[NH2:1][C:2]1[C:7]([C:8]2[CH:13]=[C:12]([F:14])[CH:11]=[C:10]([F:15])[CH:9]=2)=[C:6]([C:16](=[O:18])[CH3:17])[CH:5]=[C:4]([Cl:19])[C:3]=1[CH3:20].N1C=CC=CC=1.Cl[CH2:28][CH2:29][CH2:30][C:31](Cl)=[O:32].CC(C)([O-])C.[K+]>C(Cl)Cl.O1CCCC1>[C:16]([C:6]1[C:7]([C:8]2[CH:9]=[C:10]([F:15])[CH:11]=[C:12]([F:14])[CH:13]=2)=[C:2]([N:1]2[CH2:28][CH2:29][CH2:30][C:31]2=[O:32])[C:3]([CH3:20])=[C:4]([Cl:19])[CH:5]=1)(=[O:18])[CH3:17]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 1049PyridineHCID 783704-Chlorobutyryl chlorideHCID 23665647Potassium tert-butoxideHCID 583685171-(6-Amino-4-chloro-3',5'-difluoro-5-methylbiphenyl-2-yl)ethanone

生成物 1

HCID 866667701-(6-Acetyl-4-chloro-3',5'-difluoro-3-methylbiphenyl-2-yl)pyrrolidin-2-one収率 12.1%

試薬・触媒・溶媒 2

HCID 6344
Dichloromethane
溶媒
HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a mixture of 1-(6-amino-4-chloro-3′,5′-difluoro-5-methylbiphenyl-2-yl)ethanone (0.10 g, 0.34 mmol) and pyridine (0.041 mL, 0.51 mmol) in methylene chloride (2 mL) was added 4-chlorobutanoyl chloride (0.042 mL, 0.37 mmol). The reaction was stirred at room temperature for 1 hour, quenched with saturated sodium bicarbonate solution and extracted with ethyl acetate. The combined extracts were dried over MgSO4 and concentrated to dryness under reduced pressure. The resulting residue was treated with 1.0 M potassium tert-butoxide in tetrahydrofuran (0.84 mL, 0.84 mmol) in tetrahydrofuran (2 mL) at room temperature for 2 hours. The reaction was quenched with aq. NH4Cl, extracted with ethyl acetate. The combined organic layers were washed with water and brine, dried over MgSO4 and evaporated. The residue was purified on silica gel (eluting with 0-40% of ethyl acetate in hexanes) to give the desired product (15 mg, 12%), LCMS calculated for C19H17ClF2NO2 (M+H)+: m/z=364.1. found: 364.1.

後処理

  1. customquenched with saturated sodium bicarbonate solution
  2. extractionextracted with ethyl acetate
  3. dry with materialThe combined extracts were dried over MgSO4
  4. concentrationconcentrated to dryness under reduced pressure
  5. customThe reaction was quenched with aq. NH4Cl
  6. extractionextracted with ethyl acetate
  7. washThe combined organic layers were washed with water and brine
  8. dry with materialdried over MgSO4
  9. customevaporated
  10. customThe residue was purified on silica gel (eluting with 0-40% of ethyl acetate in hexanes)

出典と根拠

ORDレコード
ord-62fca9299ef04353baa6f7459e73d2f5
出典データセット
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09096600B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート